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WO1991011710A1 - Cellule electrolytique de detection d'analytes multiples - Google Patents

Cellule electrolytique de detection d'analytes multiples Download PDF

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Publication number
WO1991011710A1
WO1991011710A1 PCT/US1991/000358 US9100358W WO9111710A1 WO 1991011710 A1 WO1991011710 A1 WO 1991011710A1 US 9100358 W US9100358 W US 9100358W WO 9111710 A1 WO9111710 A1 WO 9111710A1
Authority
WO
WIPO (PCT)
Prior art keywords
polymer
set forth
poly
species
electrolytic sensor
Prior art date
Application number
PCT/US1991/000358
Other languages
English (en)
Inventor
Jose P. Joseph
Marc J. Madou
Original Assignee
Commtech International
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Commtech International filed Critical Commtech International
Publication of WO1991011710A1 publication Critical patent/WO1991011710A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/4162—Systems investigating the composition of gases, by the influence exerted on ionic conductivity in a liquid

Definitions

  • the present invention relates to an electrolytic cell system which is useful for determining the concentrations of an ionic species and of vaporous non-ionic species which are dissolved in a liquid.
  • a cell system can be used for detecting oxygen, carbon dioxide and hydrogen ion (pH) utilizing a single membrane.
  • Electrolytic cells have been formulated which are capable of analyzing the concentrations of vaporous analytes which are dissolved in a liquid. Such cells have been formulated on substrates by having an electrode on the substrate which is sensitive to the analyte, having an electrolyte in contact with the electrode, having an appropriate reference electrode to complete the circuit, and having a membrane covering the electrode and the electrolyte, which membrane is permeable to the vaporous analyte and impermeable to the liquid.
  • the analyte may be oxygen, carbon dioxide, hydrogen, or virtually any vaporous analyte for which an analysis is desired.
  • the permeability of the membrane can be due to small passages appropriately sized to admit the analyte and/or the analyte can dissolve in the membrane and be transported as a solute through the membrane. It is also known to analyze for ionic analytes dissolved in a liquid utilizing sensors which include a substrate with an electrode on a sensing surface thereof, an electrolyte contacting the electrode and a membrane covering the analyte and the electrode, the membrane being impervious to the liquid being analyzed but sufficiently pervious to ' a dissolved ionic analyte to allow, with the use of an appropriate ionophore, the setting up of a potential difference between the liquid and the membrane.
  • the present invention is directed to overcoming one or more of the problems as set forth above.
  • an electrolytic cell system for determining the concentrations of an ionic species and of a vaporous species, both of which are dissolved in a liquid.
  • the cell system comprises a substrate having an ionic species sensing area and a vaporous species sensing area.
  • a first electrolyte is in contact with the ionic species sensing area and a second electrolyte is in contact with the vaporous species sensing area.
  • a single membrane covers both sensing areas and both electrolytes .
  • the membrane is permeable to a first vaporous species, impermeable to the liquid, and has dispersed in it an ionophore which senses the ionic species via selective transfer into the membrane of a quantity of the ionic species determined by the concentration of the ionic species in the liquid being analyzed.
  • a first electrode is in contact with the first electrolyte.
  • a second electrode is in contact with the second electrolyte. The electrodes are free from contact with one another.
  • An electrolytic cell as set forth above has the great advantage that a single membrane acts as an ion sensitive electrode and at the same time as a volatile analyte permeable electrode whereby analysis for both components can be carried out utilizing a substrate encapsulated or covered in a single operation by the single membrane.
  • the only alternative for providing both and ionic species sensitive electrolytic cell and a volatile analyte sensitive cell on the same substrate would be to use two different membranes and to somehow seal them together or to have a portion of the substrate exposed between the two membranes . The added expense in manufacturing would be great even if the technical problems can be solved.
  • a single membrane is set forth which can be contacted with an analyte solution and can provide readouts of several parameters at once, most particularly such parameters as pH, carbon dioxide concentration and oxygen concentration. Such is particularly useful when the entire sensor can be made small and inserted in a blood vessel to provide in situ measurements of such quantities.
  • Figure 1 illustrates, in plan view, partially cut away, an electrolytic cell in accordance with the present invention
  • Figure 2 illustrates the embodiment of
  • Figure 1 in side elevation, partially in section.
  • an electrolytic cell structure 10 is set forth for determining the concentrations of both an ionic species and a vaporous species which are dissolved in a liquid, often an aqueous liquid.
  • the electrolytic cell structure 10 is built on a substrate 12 which has a first sensing area 14.
  • a first electrode 16 is on the first sensing area 14.
  • the first electrode 16 is used to determine the concentration of the ionic species.
  • the first electrode 16 is generally a common reference electrode and the potential difference is measured between the liquid being analyzed and an external electrode 18 located in the liquid being analyzed.
  • the first electrode 16 and the external electrode 18 can be of the same type, for example, both can be Ag/AgCl electrodes. The potential difference arises across the surface of the required membrane 20 which is discussed in more detail below.
  • the substrate 12 may be made of any of a number of materials.
  • the substrate 12 may be made of an insulative material, that is, a dielectric material, such as a non-conducting plastic or glass.
  • the substrate 12 can be made of a semiconducting material such as silicon or even of a conducting material so long as an appropriate dielectric material is present to electrically isolate individual cells which make up the electrolytic cell system 10.
  • the substrate 12 can be silicon having a silicon dioxide dielectric layer on it as formed by IC processing techniques. Silicon nitride or another insulative material can alternatively be used.
  • a second electrode 22 is also on the substrate 12. The second electrode 22 is capable of sensing a first vaporous species and is in contact with a second electrolyte 24.
  • the first electrode 16 and the second electrode 22 are free from contact with one another.
  • a third electrode 26 is also present on the substrate 12, is in contact with a third electrolyte 28 and is free from contact with the first electrode 16 and the second electrode 22.
  • the third electrode 26 is sensitive to a second vaporous species.
  • the second electrode 22 can be, for example, a pH sensitive electrode, e. g. , IrO,.
  • An internal reference electrode 30, for example, Ag/AgCl, is also in contact with the second electrolyte 24 and the potential difference between the electrodes 22 and 30 would indicate the concentration of the first vaporous species, e. g. , CO_ , which would pass through the membrane 20.
  • the third electrode 26 can be, for example, an Ag electrode and the internal reference electrode 32 can be Ag/AgCl with a constant voltage being applied between electrodes 26 and 32 and current being measured to determine the concentration of the second vaporous species. If the voltage is -0.7 volt and the membrane 20 is selected to be permeable to 0- , the concentration of 0_ in the liquid can be determined. It should be noted that the above discussion of specific species and electrodes is merely exemplary of the many species that are subject to analysis utilizing the apparatus and/or method of the present invention.
  • the first electrode 16, and along with it the second electrode 22, and the third electrode 30, when present, can be formulated by vapor deposition, sputtering, or the like. Generally, such techniques as are utilized in the IC art are applicable to formulate an electrolytic cell system 10 in accordance with the present invention.
  • the substrate 12, as mentioned above, may comprise any of a number of materials and its particular composition is not critical in the invention. However, it is often desirable to have a relatively small substrate 12 so that they can be utilized in situ in such positions as inside of blood vessels. Accordingly, one may make use of the techniques of the semiconductor processing art to make the electrolytic cell system 10 either on or beneath the surface of a semiconductor material, most particularly silicon. Methods for making such cells are set forth in, for example, U.S. Patent No. 4,765,864 issued August 23, 1988 to C. E. Holland, E. R. esterberg, M. J. Madou and T. Otagawa. The term ionic species is used herein to indicate any species which exists as an ion in the liquid being analyzed.
  • vaporous species is used to indicate any species which can enter the vapor state from the liquid.
  • such species include hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide, nitrous oxide, sulfur dioxide or trioxide, ammonia, hydrogen sulfide, hydrogen cyanide, hydrofluoric acid, acetic acid or halogens.
  • the electrolyte can include any of the liquids listed above having dissolved therein an appropriate ionic salt such as sodium bicarbonate, ammonium chloride, sodium nitrite, citrate buffer, potassium silver cyanide, sodium acetate, bisulfite buffer, acetate buffer, phosphate buffer, potassium or sodium chloride or generally any non-interfering salt or mixture of salts.
  • an appropriate ionic salt such as sodium bicarbonate, ammonium chloride, sodium nitrite, citrate buffer, potassium silver cyanide, sodium acetate, bisulfite buffer, acetate buffer, phosphate buffer, potassium or sodium chloride or generally any non-interfering salt or mixture of salts.
  • an appropriate ionic salt such as sodium bicarbonate, ammonium chloride, sodium nitrite, citrate buffer, potassium silver cyanide, sodium acetate, bisulfite buffer, acetate buffer, phosphate buffer, potassium or sodium chloride or generally any non-interfering salt or mixture of salts.
  • solid polymeric electrolytes besides Nafion are sulfonated styrene-divinyl benzene resins and divinyl naphthalene sulfonic acid polymer.
  • Gels useful as electrolytes for incorporation within the sensor structure include, without limitation: methylcellulose, polyvinyl alcohol, agar, carboxycellulose, gelatin, agarose, deionized gelatin, . polyacrylamide, polyvinyl pyrrolidone, hydroxyethylacrylate, hydroxyethylmethacrylate, and polyacrylic acid. They are characterized in that they constitute thickened (more viscous) solutions. They are hydrophilic in natural and include synthetic polymeric film forming materials.
  • the electrolyte can alternatively be selected from a family of inorganic oxide solid proton conductors, e.g., hydrogen uranyl phosphate, protonated ?"-alumina, zirconium phosphates or antiinonic acids.
  • a family of inorganic oxide solid proton conductors e.g., hydrogen uranyl phosphate, protonated ?"-alumina, zirconium phosphates or antiinonic acids.
  • the membrane 20 must have certain properties. First of all, it must be insoluble in the liquid. Second, it must be permeable to the vaporous species being analyzed. Third, it must be impermeable to the liquid. Fourth, it must have dispersed in it an ionophore which allows transfer into the membrane 20 of a portion of the ionic species thus setting up a potential difference at the surface of the membrane 20 which contacts the liquid sample, the magnitude of which potential difference is determined by the concentration of the ionic analyte of interest in the liquid sample.
  • the various electrodes which are useful in the method and apparatus of the invention can be any of the commonly used reference type electrodes, e. g. , silver/silver chloride or calomel electrode.
  • Electrodes 16 can also be used. These include, for example, electrodes 16 of platinum, platinum black, silver, gold, iridium, palladium, palladium/silver, " iridium dioxide, platinum black/palladium, platinum oxide, and mixtures thereof, electronically conductive polymers, pH sensitive glass electrodes, and generally any of the electrodes normally utilized in electro-chemical measurements.
  • Electrodes useful for sensing various vaporous non-ionic species may be made of silver, gold, platinum, palladium, carbon, mercury or other metals. Such electrodes can be modified with different chemicals. Selectivity is provided by the catalytic properties of the electrode and also by the potential applied to the electrodes for effecting reduction or oxidation of the non-ionic species of interest.
  • the electrode In determining acidic or basic gases, the electrode can be a pH sensing surface such as a metal oxide, pH sensitive glass or a polymer.
  • the membrane was cast upon a silicon substrate having electrodes in wells on the surface. Aqueous gel electrolytes were positioned over the electrodes prior to the casting. The solvent was allowed to evaporate for at least 24 hours. For pH and ion measurements the sensors were conditioned by contact with a solution of the appropriate ion for 10 to 24 hours.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

On présente un détecteur électrolytique destiné à mesurer les quantités d'espèces ioniques et sous forme de vapeur contenues dans un liquide. Le système possède une électrode (16) sensible à une espèce ionique et une autre électrode (22) sensible à une espèce sous forme de vapeur. Une membrane unitaire (20) recouvre les électrodes et l'électrolyte nécessaire, cette membrane étant perméable à l'espèce sous forme de vapeur et imperméable au liquide et contenant un ionophore en dispersion qui détecte l'espèce ionique par transfert sélectif à travers la membrane d'une quantité de l'espèce ionique déterminée par la concentration de l'espèce ionique dans le liquide. Des quantités telles que les concentrations d'ions hydrogène, de dioxyde de carbone et d'oxygène peuvent être déterminées par une seule cellule électrolytique.
PCT/US1991/000358 1990-01-26 1991-01-17 Cellule electrolytique de detection d'analytes multiples WO1991011710A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US470,954 1990-01-26
US07/470,954 US5183549A (en) 1990-01-26 1990-01-26 Multi-analyte sensing electrolytic cell

Publications (1)

Publication Number Publication Date
WO1991011710A1 true WO1991011710A1 (fr) 1991-08-08

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Family Applications (1)

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PCT/US1991/000358 WO1991011710A1 (fr) 1990-01-26 1991-01-17 Cellule electrolytique de detection d'analytes multiples

Country Status (4)

Country Link
US (1) US5183549A (fr)
EP (1) EP0512070A4 (fr)
CA (1) CA2074511A1 (fr)
WO (1) WO1991011710A1 (fr)

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EP0588153A1 (fr) * 1992-09-14 1994-03-23 Siemens Aktiengesellschaft Capteur de gaz
WO1995022052A1 (fr) * 1994-02-11 1995-08-17 Ecossensors Limited Detection de la presence de plomb dans le sang
EP0772043A2 (fr) 1995-10-31 1997-05-07 Ciba Corning Diagnostics Corp. Joint en fluoroélastomère pour capteurs d'analytes dans le sang
DE19628052C1 (de) * 1996-07-11 1997-11-27 Fraunhofer Ges Forschung Sensor- und/oder Trennelement sowie Verfahren zu dessen Herstellung und Anwendung desselben
EP0810431A1 (fr) * 1996-05-31 1997-12-03 Siemens Aktiengesellschaft Capteur électrochimique
US5804049A (en) * 1993-09-15 1998-09-08 Chiron Diagnostics Corporation Material for establishing solid state contact for ion selective electrodes
US5911862A (en) * 1993-09-15 1999-06-15 Chiron Diagnostics Corporation Material for establishing solid state contact for ion selective electrodes
WO1999030144A1 (fr) * 1997-12-11 1999-06-17 The Victoria University Of Manchester Dispositifs de detection et procede d'analyse
DE10214713A1 (de) * 2002-04-03 2003-10-30 C Cit Ag Waedenswill Vorrichtung und Verfahren zur Durchführung und zur kontinuierlichen Überwachung von chemischen und/oder biologischen Reaktionen
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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0588153A1 (fr) * 1992-09-14 1994-03-23 Siemens Aktiengesellschaft Capteur de gaz
US5804049A (en) * 1993-09-15 1998-09-08 Chiron Diagnostics Corporation Material for establishing solid state contact for ion selective electrodes
US6416646B2 (en) 1993-09-15 2002-07-09 Bayer Corporation Method of making a material for establishing solid state contact for ion selective electrodes
US6251246B1 (en) 1993-09-15 2001-06-26 Bayer Corporation Material for establishing solid state contact for ion selective electrodes
US5911862A (en) * 1993-09-15 1999-06-15 Chiron Diagnostics Corporation Material for establishing solid state contact for ion selective electrodes
US5814205A (en) * 1994-02-11 1998-09-29 Palintest Limited Detection of lead in blood
AU692830B2 (en) * 1994-02-11 1998-06-18 Palintest Limited Detection of lead in blood
WO1995022052A1 (fr) * 1994-02-11 1995-08-17 Ecossensors Limited Detection de la presence de plomb dans le sang
EP0772043A3 (fr) * 1995-10-31 1998-04-22 Ciba Corning Diagnostics Corp. Joint en fluoroélastomère pour capteurs d'analytes dans le sang
EP0772043A2 (fr) 1995-10-31 1997-05-07 Ciba Corning Diagnostics Corp. Joint en fluoroélastomère pour capteurs d'analytes dans le sang
EP0810431A1 (fr) * 1996-05-31 1997-12-03 Siemens Aktiengesellschaft Capteur électrochimique
US5900128A (en) * 1996-05-31 1999-05-04 Siemens Aktiengesellschaft Electrochemical sensor
DE19628052C1 (de) * 1996-07-11 1997-11-27 Fraunhofer Ges Forschung Sensor- und/oder Trennelement sowie Verfahren zu dessen Herstellung und Anwendung desselben
WO1999030144A1 (fr) * 1997-12-11 1999-06-17 The Victoria University Of Manchester Dispositifs de detection et procede d'analyse
DE10214713A1 (de) * 2002-04-03 2003-10-30 C Cit Ag Waedenswill Vorrichtung und Verfahren zur Durchführung und zur kontinuierlichen Überwachung von chemischen und/oder biologischen Reaktionen
DE10300957A1 (de) * 2003-01-13 2004-07-22 Ibidi Gmbh Probenkammer für eine Flüssigkeit

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EP0512070A4 (en) 1993-06-09
US5183549A (en) 1993-02-02
CA2074511A1 (fr) 1991-07-27
EP0512070A1 (fr) 1992-11-11

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